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1.
Feth MP Bolm C Hildebrand JP Köhler M Beckmann O Bauer M Ramamonjisoa R Bertagnolli H 《Chemistry (Weinheim an der Bergstrasse, Germany)》2003,9(6):1348-1359
XANES and EXAFS spectroscopic studies at the Mn-K- and Br-K-edge of reaction products of (S,S)-(+)-N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediaminomanganese(III) chloride ([(salen)Mn(III)Cl], 1) and (S,S)-(+)-N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediaminomanganese(III) bromide ([(salen)Mn(III)Br], 2) with 4-phenylpyridine N-oxide (4-PPNO) and 3-chloroperoxybenzoic acid (MCPBA) are reported. The reaction of the Mn(III) complexes with two equivalents of 4-PPNO leads to a hexacoordinated compound, in which the manganese atom is octahedrally coordinated by four oxygen/nitrogen atoms of the salen ligand at an average distance of approximately 1.90 A and two additional, axially bonded oxygen atoms of the 4-PPNO at 2.25 A. The oxidation state of this complex was determined as approximately +IV by a comparative study of Mn(III) and Mn(V) reference compounds. The green intermediate obtained in reactions of MCPBA and solutions of 1 or 2 in acetonitrile was investigated with XANES, EXAFS, UV/Vis, and Raman spectroscopy, and an increase of the coordination number of the manganese atoms from 4 to 5 and the complete abstraction of the halide was observed. A formal oxidation state of IV was deduced from the relative position of the pre-edge 1s-->3d feature of the X-ray absorption spectrum of the complex. The broad UV/Vis band of this complex in acetonitrile with lambda(max)=648 nm was consistent with a radical cation structure, in which a MCPBA molecule was bound to the Mn(IV) central atom. An oxomanganese(V) or a dimeric manganese(IV) species was not detected. 相似文献
2.
Feth Martin P. Weber Achim Merkle Rotraut Reinöhl Ulrich Bertagnolli Helmut 《Journal of Sol-Gel Science and Technology》2003,27(2):193-204
Two solid solutions of lead zirconium titanates PbZr
x
Ti1 – x
O3 (x = 0.1 and 0.35) as well as the reference compounds lead titanate and lead zirconate were prepared from zirconium and titanium n-propoxide, dissolved in 2-methoxyethanol, by sol-gel process. The amorphous products after pyrolysis of the dried gels and the crystalline phases were studied by EXAFS spectroscopy to monitor the structural changes from the amorphous oxide mixture to the crystalline ceramics after calcination. Additionally, the crystalline phases were identified by X-ray diffraction (XRD).It follows from the analysis of the EXAFS data that the local order of the amorphous phases seems to be completely different from that of the crystalline phase. There is no indication of a preformation of the local order of the perovskite structure. The analysis of our EXAFS spectra can be interpreted very consistently with the assumption that in the amorphous samples a segregation exists on molecular level and the low crystallisation temperatures are a consequence of very short diffusion paths. 相似文献
3.
R D Chambers L L Feth E M Burns 《The Journal of the Acoustical Society of America》1986,80(6):1673-1680
The relation between the auditory brain stem potential called the frequency-following response (FFR) and the low pitch of complex tones was investigated. Eleven complex stimuli were synthesized such that frequency content varied but waveform envelope periodicity was constant. This was accomplished by repeatedly shifting the components of a harmonic complex tone upward in frequency by delta f of 20 Hz, producing a series of six-component inharmonic complex tones with constant intercomponent spacing of 200 Hz. Pitch-shift functions were derived from pitch matches for these stimuli to a comparison pure tone for each of four normal hearing adults with extensive musical training. The FFRs were recorded for the complex stimuli that were judged most divergent in pitch by each subject and for pure-tone signals that were judged equal in pitch to these complex stimuli. Spectral analyses suggested that the spectral content of the FFRs elicited by the complex stimuli did not vary consistently with component frequency or the first effect of pitch shift. Furthermore, complex and pure-tone signals judged equal in pitch did not elicit FFRs of similar spectral content. 相似文献
4.
A discussion is given of the relation between the maximum functionaltheorem and Schwinger's variational principle, and it is shownthat the bound given by Schwinger's principle is better thanor the same as that given by the maximum functional theorem. 相似文献
5.
6.
7.
Meier R Maigut J Kallies B Lehnert N Paulat F Heinemann FW Zahn G Feth MP Krautscheid H van Eldik R 《Chemical communications (Cambridge, England)》2007,(38):3960-3962
The equilibrium between the twist-boat (tb) and half-chair (hc) conformers of the central diamine chelate ring of [Fe(III)(tmdta)]- in solids and aqueous solution has been studied by Raman spectroscopy, supported by calculated Raman spectra using Density Functional Theory. 相似文献
8.
Bolm C Martin M Gescheidt G Palivan C Stanoeva T Bertagnolli H Feth M Schweiger A Mitrikas G Harmer J 《Chemistry (Weinheim an der Bergstrasse, Germany)》2007,13(6):1842-1850
The initial steps of an enantioselective Diels-Alder reaction catalyzed by a CuII-bissulfoximine complex were followed by EXAFS (EXAFS=extended X-ray absorption fine structure), EPR (EPR=electron paramagnetic resonance) spectroscopy (CW-EPR, FID-detected EPR, pulse ENDOR, HYSCORE; CW=continuous wave; ENDOR=electron nuclear double resonance; HYSCORE=hyperfine sublevel correlation; FID=free induction decay), and UV-visible spectroscopy. The complexes formed between the parent CuX2 (X=Cl-, Br-, TfO-, SbF6-) salts, the chiral bissulfoximine ligand (S,S)-1, and N-(1-oxoprop-2-en-1-yl)oxazolidin-2-one (2) as the substrate in CH2Cl2 were investigated in frozen and fluid solution. In all cases, penta- or hexacoordinated CuII centers were established. The complexes with counterions indicating high stereoselectivity (TfO- and SbF6-) reveal one unique species in which substrate 2 binds to pseudoequatorial positions (via O atoms), shifting the counterions to axial locations. On the other hand, those lacking stereoselectivity (X=Cl- and Br-) form two species in which the parent halogen anions remain at equatorial positions preventing the formation of geometries compatible with those found for X=TfO- and SbF6-. 相似文献
9.
Van Zandt LL 《Physical review letters》1986,57(16):2085-2087
10.
Alumina- (5 and 10 wt%) doped zirconia samples were prepared by sol-gel processing of aluminum sec-butoxide and zirconium butoxide in the presence of acids (acetic, sulfuric or nitric acid) or organic additives (Pluronic P123). X-ray absorption spectroscopy, X-ray diffraction and nitrogen adsorption experiments showed that the structure of the synthesized mixed oxides is strongly influenced by the chemical synthesis parameters. 相似文献